Preparation method of scopolamine butylbromide

A technology of scopolamine and scopolamine, which is applied in the field of preparation of scopolamine butylbromide, can solve the problems of no application value, low method yield and high price, and achieves the effects of easy recovery and processing, high yield and low cost

Active Publication Date: 2011-08-10
LAKERSPHARMA CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] The method (2) has a low yield and has no application value. It is reported that scopolamine butylbromide mostly adopts the method (1) at present.
[0008] However, although the process of (1) method is relatively mature, the yield is still on the low side and the cost is high, especially when acetonitrile is used as the reaction medium, the price is high and the dosage is large, and acetonitrile is a first-class flammable liquid, which is toxic and poses a threat to safety. Production and environmental protection bring certain pressure

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  • Preparation method of scopolamine butylbromide

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Embodiment Construction

[0024] The present invention will be further described below in conjunction with specific implementation examples.

[0025] (1) Preparation of crude scopolamine butylbromide

[0026] Add 10 grams (0.033 moles) of scopolamine to a 100ml round bottom flask equipped with a glass condenser,

[0027] 30ml (0.278 moles) of n-butane bromide was stirred, heated in a water bath, and refluxed at 90°C for 30 hours. After the reaction is complete, cool the reactant to room temperature, remove the oily liquid, concentrate the residue to dryness under reduced pressure at 75°C, add 30ml of absolute ethanol, heat to dissolve, place at room temperature, precipitate crystals and place in the refrigerator (8~10°C) overnight. After filtering, the crystals were washed with absolute ethanol, sucked dry, and dried under vacuum at 70°C for 4 hours to obtain 9.6 g of crude scopolamine butylbromide.

[0028] (2) refined

[0029] Add 9.6g of crude scopolamine butylbromide and 45ml of absolute ethano...

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Abstract

The invention discloses a preparation method of scopolamine butylbromide, comprising the steps of: (1) subjecting scopolamine and n-butyl bromide to heating under reflux to complete reaction; (2) preparing a crude product of scopolamine butylbromide; and (3) refining the crude product of scopolamine butylbromide. By means of the invention, by utilizing the physicochemical property that n-butyl bromide has excellent dissolubility for scopolamine, but poor dissolubility for reaction product scopolamine butylbromide, the scopolamine and excessive n-butyl bromide are reacted, and thus the yield of scopolamine butylbromide is improved by raising reaction temperature, increasing reaction speed and shortening reaction time. In the preparation method of scopolamine butylbromide, disclosed by the invention, the use of any medium is avoided, the n-butyl bromide is not only used as a raw material for synthesizing scopolamine butylbromide, but also as a reaction solvent with stable properties, excessive n-butyl bromide can be recovered and treated relatively easily after the reaction is finished and can be repeatedly used, and thus, cost reduction is facilitated, and environment is protected.

Description

technical field [0001] The invention relates to a preparation method of scopolamine butylbromide. Background technique [0002] Scopolamine butylbromide is a peripheral anticholinergic drug developed by Boehringer in Germany and launched in February 1956. The drug is used for gastrointestinal spasm, biliary colic, renal colic or hyperperistalsis of the gastrointestinal tract caused by various etiologies. In addition, the drug is also clinically used for preoperative preparation of gastric, duodenum, and colonic fiber endoscopy, endoscopic retrograde cholangiopancreatography, and barium hypotonic angiography or CT of gastroduodenum and colon. Preoperative preparation for scanning, which reduces or inhibits gastrointestinal motility, is a commonly used antispasmodic drug for the digestive system. [0003] The preparation method of Scopolamine Butylbromide of bibliographical information mainly contains following two kinds: [0004] (1) Using acetonitrile as the reaction medi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D451/10
Inventor 林英昌冯锦玲
Owner LAKERSPHARMA CO LTD
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